超高效液相色谱-串联质谱法同时测定食品中双酚A和双酚S
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摘要
采用超高效液相色谱-串联质谱法同时测定食品中双酚A和双酚S的含量。食品样品经乙腈提取和石墨化炭黑吸附剂固相萃取柱净化。以Waters BEH C_(18)色谱柱为分离柱,以不同体积比的水和甲醇的混合液为流动相进行梯度洗脱,采用电喷雾负离子源和多反应监测模式检测。采用同位素内标法定量。双酚A和双酚S的线性范围依次为1.04~52.0,0.23~11.65μg·L~(-1),检出限(3S/N)依次为0.30,0.10μg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为94.6%~101%,测定值的相对标准偏差(n=6)为2.5%~6.6%。
UHPLC-MS/MS was applied to the simultaneous determination of bisphenol A and bisphenol S in foods.The food sample was extracted with acetonitrile and purified with GCB solid phase extraction column.Waters BEH C_(18) chromatographic column was used as stationary phase,and the mixture of water and methanol mixed in different ratios was used as mobile phase in gradient elution.ESI-and multi-reactions monitor mode were adopted in MS/MS.Isotope was used as internal standard.Linearity ranges of bisphenol A and bisphenol S were found in the range of 1.04-52.0,0.23-11.65μg·L~(-1) respectively,with detection limits(3 S/N)of 0.30,0.10μg·kg~(-1) respectively.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 94.6%-101%,with RSD′s(n=6)in the range of 2.5%-6.6%.
UHPLC-MS/MS was applied to the simultaneous determination of bisphenol A and bisphenol S in foods.The food sample was extracted with acetonitrile and purified with GCB solid phase extraction column.Waters BEH C_(18) chromatographic column was used as stationary phase,and the mixture of water and methanol mixed in different ratios was used as mobile phase in gradient elution.ESI-and multi-reactions monitor mode were adopted in MS/MS.Isotope was used as internal standard.Linearity ranges of bisphenol A and bisphenol S were found in the range of 1.04-52.0,0.23-11.65μg·L~(-1) respectively,with detection limits(3 S/N)of 0.30,0.10μg·kg~(-1) respectively.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 94.6%-101%,with RSD′s(n=6)in the range of 2.5%-6.6%.
引文
[1]ASIMAKOPOULOS A G,THOMAIDIS N S,KOUPPARIS M A.Recent trends in biomonitoring of bisphenol A,4-t-octylphenol,and 4-nonylphenol[J].Toxicology Letters,2012,210(2):141-154.
[2]VOM SAAL F S,NAGEL S C,COE B L,et al.The estrogenic endocrine disrupting chemical bisphenol A(BPA)and obesity[J].Molecular and Cellular Endocrinology,2012,354(1/2):74-84.
[3]LAKIND J S,NAIMAN D Q.Temporal trends in bisphenol A exposure in the United States from 2003-2012and factors associated with BPA exposure:Spot samples and urine dilution complicate data interpretation[J].Environmental Research,2015,142:84-95.
[4]PFEIFER D,CHUNG Y M,HU M C.Effects of lowdose bisphenol A on DNA damage and proliferation of breast cells:The role of c-Myc[J].Environmental Health Perspectives,2015,123(12):1271-1279.
[5]MUSTIELES V,PREZ-LOBATO R,OLEA N,et al.Bisphenol A:Human exposure and neuro-behavior[J].Neurotoxicology,2015,49:174-184.
[6]陈宗保,刘林海,董洪霞.基于双重增敏剂荧光法测定食品包装材料中痕量双酚A[J].化学研究与应用,2016,28(6):829-832.
[7]张秋菊,曹林波,翁少梅,等.固相微萃取-高效液相色谱法测定牛奶和肉类中己烯雌酚、丙酸睾酮和双酚A[J].中国卫生检验杂志,2017,27(5):635-638.
[8]蔡言红,彭辉,裴晓洋,等.磁性竹炭为吸附剂的分散基质固相萃取分离-高效液相色谱法测定水中双酚S的含量[J].理化检验-化学分册,2017,53(10):1151-1155.
[9]李勇竞.微波消解-固相萃取-气相色谱-质谱联用法测定泡沫快餐盒中的双酚A[J].中国食品卫生杂志,2013,25(4):344-347.
[10]李少霞,黄伟雄,余胜兵,等.气相色谱-质谱法测定奶瓶中双酚A含量[J].理化检验-化学分册,2013,49(6):679-682.
[11]王军淋,陆亚亚,张念华,等.超高效液相色谱-串联质谱法快速测定纸质食品包装材料及容器中的7种双酚类化合物[J].中国卫生检验杂志,2017,27(13):1858-1861.
[12]潘胜东,何仟,陈晓红,等.固相萃取-超高效液相色谱-高分辨质谱法快速测定食用油中4种酚类环境雌激素残留[J].色谱,2017,9(35):980-986.
[13]李蔚,赵秀香,李凤华.超高效液相色谱-串联质谱法检测婴幼儿乳粉中双酚A和壬基酚[J].预防医学论坛,2017,23(3):233-235.
[14]潘衍宇,安康,赵雪桢,等.泰安市售130份塑料包装饮料双酚A含量检测及膳食风险评估[J].现代预防医学,2017,44(20):3684-3701.
[15]陈玫宏,郭敏,刘丹,等.典型内分泌干扰物在太湖及其支流水体和沉积物中的污染特征[J].中国环境科学,2017,37(11):4323-4332.
[16]叶超,刘燕群,游浩.武汉地区水中环境内分泌干扰物的污染情况及其对人体的影响[J].职业与健康,2013,29(7):880-882.
[17]吴皓,孙东,蔡卓平,等.双酚A的内分泌干扰效应研究进展[J].生态科学,2017,36(3):200-206.
[18]严燕,黄蔷,牟敬锋.桶装饮用水中双酚A的二次污染调查及暴露评估[J].实用预防医学,2017,24(1):43-45.
[2]VOM SAAL F S,NAGEL S C,COE B L,et al.The estrogenic endocrine disrupting chemical bisphenol A(BPA)and obesity[J].Molecular and Cellular Endocrinology,2012,354(1/2):74-84.
[3]LAKIND J S,NAIMAN D Q.Temporal trends in bisphenol A exposure in the United States from 2003-2012and factors associated with BPA exposure:Spot samples and urine dilution complicate data interpretation[J].Environmental Research,2015,142:84-95.
[4]PFEIFER D,CHUNG Y M,HU M C.Effects of lowdose bisphenol A on DNA damage and proliferation of breast cells:The role of c-Myc[J].Environmental Health Perspectives,2015,123(12):1271-1279.
[5]MUSTIELES V,PREZ-LOBATO R,OLEA N,et al.Bisphenol A:Human exposure and neuro-behavior[J].Neurotoxicology,2015,49:174-184.
[6]陈宗保,刘林海,董洪霞.基于双重增敏剂荧光法测定食品包装材料中痕量双酚A[J].化学研究与应用,2016,28(6):829-832.
[7]张秋菊,曹林波,翁少梅,等.固相微萃取-高效液相色谱法测定牛奶和肉类中己烯雌酚、丙酸睾酮和双酚A[J].中国卫生检验杂志,2017,27(5):635-638.
[8]蔡言红,彭辉,裴晓洋,等.磁性竹炭为吸附剂的分散基质固相萃取分离-高效液相色谱法测定水中双酚S的含量[J].理化检验-化学分册,2017,53(10):1151-1155.
[9]李勇竞.微波消解-固相萃取-气相色谱-质谱联用法测定泡沫快餐盒中的双酚A[J].中国食品卫生杂志,2013,25(4):344-347.
[10]李少霞,黄伟雄,余胜兵,等.气相色谱-质谱法测定奶瓶中双酚A含量[J].理化检验-化学分册,2013,49(6):679-682.
[11]王军淋,陆亚亚,张念华,等.超高效液相色谱-串联质谱法快速测定纸质食品包装材料及容器中的7种双酚类化合物[J].中国卫生检验杂志,2017,27(13):1858-1861.
[12]潘胜东,何仟,陈晓红,等.固相萃取-超高效液相色谱-高分辨质谱法快速测定食用油中4种酚类环境雌激素残留[J].色谱,2017,9(35):980-986.
[13]李蔚,赵秀香,李凤华.超高效液相色谱-串联质谱法检测婴幼儿乳粉中双酚A和壬基酚[J].预防医学论坛,2017,23(3):233-235.
[14]潘衍宇,安康,赵雪桢,等.泰安市售130份塑料包装饮料双酚A含量检测及膳食风险评估[J].现代预防医学,2017,44(20):3684-3701.
[15]陈玫宏,郭敏,刘丹,等.典型内分泌干扰物在太湖及其支流水体和沉积物中的污染特征[J].中国环境科学,2017,37(11):4323-4332.
[16]叶超,刘燕群,游浩.武汉地区水中环境内分泌干扰物的污染情况及其对人体的影响[J].职业与健康,2013,29(7):880-882.
[17]吴皓,孙东,蔡卓平,等.双酚A的内分泌干扰效应研究进展[J].生态科学,2017,36(3):200-206.
[18]严燕,黄蔷,牟敬锋.桶装饮用水中双酚A的二次污染调查及暴露评估[J].实用预防医学,2017,24(1):43-45.